Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of silicon nitride single crystal and its preparation method and application

A technology of silicon nitride single crystal and nitrogen source, applied in the field of semiconductors, can solve the problems of low purity of silicon nitride, complicated process and great human injury, and achieve the effects of safe operation, simple steps and good quality.

Active Publication Date: 2022-04-08
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are still various deficiencies in the preparation of silicon nitride at present. For example, patent CN104891455A discloses a method for preparing silicon nitride nanomaterials, which is mainly by placing a mixture of silicon tetrachloride and lithium nitride in a special stainless steel reactor and Sealed, heated in a resistance crucible furnace, the product is washed with alcohol, pickled and water until neutral, separated and dried to obtain silicon nitride nanomaterials, but this method uses silicon tetrachloride as raw material to prepare silicon nitride, tetrachloride Silicon is very harmful to the human body and is likely to cause environmental pollution; Yang et al. (Ultra-Long Single-Crystalline Alpha-Si 3 N 4 Nanowires: Derived Froma Polymeric Precursor [J]. Journal of the American Ceramic Society, 2005, 88 (6): 1647-1650) uses liquid polysilazane as a raw material, which is first cured at 260°C, then taken out and ground and mixed with FeCl 2 Mix well and react under nitrogen at 1250°C to obtain single crystal nanowires of good quality. However, in comparison experiments, it was found that no nanowires would be formed without the addition of catalysts, and metal elements were introduced as catalysts. The purity of silicon nitride was low, which caused great harm to purification. Difficulty, complicated process; Lin et al. (Synthesis and optical property of ultra-long alpha-Si 3 N 4 nanowires under superatmospheric pressure conditions[J]. Crystengcomm, 2012, 14(9): 3250-3256) with methane as reducing gas, nitrogen as nitrogen source, SiO or Si and SiO 2 The mixed substance is used as the silicon source, nitrogen and argon are used as the carrier gas, and high-quality silicon nitride nanowires are grown by CVD under the conditions of pressurization (1.1-1.5atm) and 1400-1550°C, but this method contains methane and other flammable materials. Gas, harsh reaction conditions, such as high temperature of 1500 ° C, need to pressurize, etc., resulting in low operating safety and high requirements for equipment; patent CN108059133A discloses a nano-silicon nitride and its preparation method, which is to process silicate Ball milling to obtain powdered silicate, and mix it with magnesium powder, magnesium chloride, and ammonium chloride to obtain a mixture, and then heat the obtained mixture to 800-1000°C at a heating rate of 8-20°C / min and keep it for 6 ~18h, pickling after cooling to obtain nano-silicon nitride, but the nano-silicon nitride particles prepared by ball milling method are not uniform

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of silicon nitride single crystal and its preparation method and application
  • A kind of silicon nitride single crystal and its preparation method and application
  • A kind of silicon nitride single crystal and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0028] An aspect of the embodiments of the present invention provides a method for preparing a silicon nitride single crystal, which includes:

[0029] Provide SiC substrate;

[0030] Arranging multi-layer graphene as an intercalation layer on the SiC substrate to obtain a graphene / SiC substrate;

[0031] And, the graphene / SiC substrate is placed in the reaction chamber of the epitaxial growth equipment, a gaseous nitrogen source is introduced into the reaction chamber and epitaxial growth is carried out, so as to obtain a silicon nitride single crystal.

[0032] In some more specific embodiments, the SiC substrate includes any one of a 2H-SiC substrate, a 3C-SiC substrate, a 4H-SiC substrate, and a 6H-SiC substrate, and is not limited thereto.

[0033] Further, the SiC substrate includes a SiC substrate with a chamfered surface.

[0034] Further, the thickness of the multi-layer graphene is 0.34-3.4 nm.

[0035] Further, the number of layers of the multi-layer graphene is ...

Embodiment 1

[0061] (1) Using 6H-SiC as the substrate, directly epitaxially grow 2.04nm (6 layers) graphene as the insertion layer on the 6H-SiC substrate;

[0062] (2) Put the 6H-SiC substrate grown with multilayer graphene into the reaction chamber, and first pass H 2 The surface of the graphene / SiC substrate was cleaned at 1050°C for 10 minutes, and H 2 The rate is 17.5slm;

[0063] (3) Feed NH with a flow rate of 2.0L / min into the reaction chamber 3 As a nitrogen source, the growth temperature is 1100°C, the growth time is 10h, and Si 3 N 4 single crystal particles.

[0064] Si prepared in this example 3 N 4 Scanning electron microscope images of single crystal particles such as image 3 As shown, the atomic force microscope image as Figure 4 As shown, the energy spectrum is characterized as Figure 5 Shown; Si prepared in this embodiment 3 N 4 A spherical aberration-corrected transmission electron microscope image of a single crystal grain as Figure 6a-Figure 6b As shown...

Embodiment 2

[0066] (1) Using 4H-SiC as the substrate, directly epitaxially grow 3.4nm (10 layers) graphene as an insertion layer on the 4H-SiC substrate;

[0067] (2) Put the 4H-SiC substrate grown with 10 layers of graphene into the reaction chamber, and first pass H 2 The surface of the graphene / SiC substrate was cleaned at 900°C for 10 minutes, and H 2 The rate is 15slm;

[0068] (3) Feed NH with a flow rate of 2L / min into the reaction chamber 3 As a nitrogen source, the growth temperature is 1000°C, the growth time is 50h, and Si 3 N 4 single crystal particles.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
thicknessaaaaaaaaaa
lengthaaaaaaaaaa
diameteraaaaaaaaaa
Login to View More

Abstract

The invention discloses a silicon nitride single crystal, its preparation method and application. The preparation method includes: using epitaxial growth method to directly epitaxially grow multilayer graphene as an insertion layer on a SiC substrate to obtain a graphene / SiC substrate; and, placing the graphene / SiC substrate on In the reaction chamber of the epitaxial growth equipment, a gaseous nitrogen source is introduced into the reaction chamber for epitaxial growth, thereby producing a silicon nitride single crystal. The method for preparing silicon nitride single crystals in the present invention does not need to add additional silicon sources, the steps are simple, the operation is safe, and can be peeled off and transferred together with graphene; at the same time, the silicon nitride single crystal particles prepared by the present invention have high uniformity and good quality. The residual stress is small.

Description

technical field [0001] The invention belongs to the technical field of semiconductors, and in particular relates to a silicon nitride single crystal and its preparation method and application. Background technique [0002] Silicon nitride material has excellent high temperature performance, such as high strength, high hardness, good wear resistance, thermal shock resistance and oxidation resistance, and also has corrosion resistance and high chemical stability. It is widely used in metallurgical refractory, Aerospace and ceramic composite materials. And similar to III-N compounds such as GaN and AlN, silicon nitride is also a wide-bandgap semiconductor (5.3eV) with a high doping level, and its electrical and electronic properties can be adjusted by reducing its energy band by doping and other means. Optical properties, so as to prepare electronic devices that can be used in high temperature and high radiation environments. [0003] Nanostructures have the characteristics o...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/38C30B25/18
CPCC30B29/38C30B25/186
Inventor 王钰宁徐俞王建峰徐科
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI